沃替西汀盐晶体结构及理化性质

沃替西汀(VOT)是一种治疗重度抑郁症的抗抑郁药,由于其水溶性低,限制了其生物利用度和疗效,期望通过成盐方式来改善沃替西汀的水溶性。利用溶剂缓慢挥发法成功制备了2种沃替西汀盐〔沃替西汀-2-吡啶甲酸(2PA)盐(VOT-2PA)和沃替西汀-异烟酸(4PA)盐一水合物(VOT-4PA·H_2O)〕,并通过单晶X衍射数据确定了它们的晶体结构。结果表明,VOT-2PA和VOT-4PA·H_2O具有相似的N—H…O氢键基础框架。并对晶体结构进行了Hirshfeld表面计算,以便从微观结构深入了解弱作用力之间的差异。利用红外光谱、差式扫描量热法和粉末X射线衍射对2种沃替西汀盐进行了表征和分析。与沃替西汀原料药相比,2种新盐均表现出更好的热稳定性和溶解度。结果表明,VOT-2PA和VOT-4PA·H_2O均具有改变VOT理化性质的能力。     

沃替西汀-水杨酸水合物的制备方法探究

沃替西汀(VOT)是一种新型抗抑郁药物,由于其水溶性低(0.1 mg/mL),上市的药品为其氢溴酸盐。本文期望通过药物固态化学改善沃替西汀的溶解度,从而开发出沃替西汀新盐型。研究发现VOT与乙酰水杨酸(ASA)在甲醇∶水(2∶1)中析晶出沃替西汀-水杨酸水合物(VOT-SA-0.5H_2O);进一步探究发现溶剂水并不能诱导VOT-SA盐转化成VOT-SA-0.5H_2O盐。该发现为VOT-SA盐的结晶工艺提供生产保障。     

几种吡啶类化合物的合成工艺概况

1 吡啶甲酸^[1] 吡啶甲酸包括α，β，γ-三种异构体。α-吡啶甲酸称皮考啉酸，β-吡啶甲酸俗称烟酸，γ-吡啶甲酸又叫异烟酸。它们都是医药、农药和染料的中间体。异烟酸的衍生物异烟酰肼（雷米封）和异烟酰腙用做抗结核药物。烟酸存在于生物体内，它与蛋白质结合，形成辅酶，参与机体的氧化-还原作用，促进新陈代谢。动物得不到足够的烟酸不能很好制造辅酶，     

吡啶甲酸的合成及其用途

吡啶甲酸包括异烟酸、烟酸和2-吡啶甲酸。总结了异烟酸及其同分异构体的性能和主要用途,论述了氧化剂氧化法、催化氧化法和电氧化法合成异烟酸及其同分异构体的研究现状与最新进展,展望了采用电化学原位谱学技术从分子水平研究、表征吡啶甲酸电合成反应机理,建立电合成吡啶甲酸新思路的前景。     

压力对尼龙101O凝聚态结构的影响

研究了尼龙（PA）1010在250℃，不同压力下退火30min后凝聚态结构的变化。结果表明，在压力小于1.0GPa和大于1．2GPa的范围内，PA1010室温结晶的三斜晶系的晶体结构有变化，但是（100）晶面的衍射强度随压力的增加而减弱，而（110／010）晶面的衍射强度增加；当压力在1.0-1.2GPa时，PA1010的X射线衍射图谱没有明显的衍射峰，DSC和溶解实验证实，PA1010在该压力范围内雪生了交联，并进一步讨论了PA1010在高压下发生交联的机理。     

一种新型卡马西平共晶的合成及表征

以卡马西平（CBZ）作为药物活性成分（API）,以没食子酸甲酯（MTG）作为共晶形成物（CCF）,在室温条件下制得一种新的药物共晶CBZ-MTG。通过X-射线单晶衍射测得了其晶体结构,并进行了红外光谱、X-射线粉末衍射、热重分析和差示扫描量热的表征。此外,利用HPLC测得其溶解性质并测试了稳定性,其共晶在溶解性,稳定性和生物利用度上都有了明显的改观。各种结构性质的表征,为其在药物领域的应用提供了基础数据和理论基础,为卡马西平-没食子酸甲酯共晶化合物作为药物应用及在制剂领域提供了新的选择。     

1，1-二（2-噻吩基）-1，4丁二醇晶体的合成、晶体培养及表征

合成了1,1-二（2-噻吩基）-1,4丁二醇,并在单一溶剂中得到了适合于X-射线衍射的单晶。测定了其晶体结构,用元素分析、红外光谱等对其进行了化学表征。     

一种铜配位聚合物[Cu(C_6H_4NO_2)(μ-Cl)]_n的合成、晶体结构及热稳定性

以止血环酸和2-吡啶甲醛为反应底物,采用溶剂热法,合成了一种新颖的配位聚合物[Cu(C6H4NO2)(μ-Cl)]n(C6H4NO2H=2-吡啶甲酸)。利用红外光谱、X-射线单晶衍射、热重分析对配合物结构进行了表征。结果表明:配位聚合物为四方晶系,空间群为P 42/n,晶胞参数:a=9.774(4)?,b=9.774(4)?,c=15.029(6)?,V=1435.7(11)?3,Z=16。在配位聚合物中,每个Cu2+离子与来自两个2-吡啶甲酸的3个O原子和1个N原子及2个Cl原子配位形成畸变的八面体构型。此外,每2个Cu2+通过2个Cl原子桥联形成二维网格状结构,层与层之间又通过π-π堆积和氢键作用,把二维网格状结构进一步堆积成三维超分子结构,从而更加稳定了晶体结构。     

抗抑郁药沃替西汀治疗抑郁症的进展情况

抑郁症临床上发生率高,疗效低,预后差,复发率高,目前主要治疗方法包括药物疗法、心理干预、物理疗法.药物疗法是抑郁症中度以上的主要疗法.沃替西汀是一种新的抗抑郁剂,被美国食品药物监督管理局准许用于治疗成人抑郁.概括了抗抑郁药沃替西汀治疗抑郁症相关情况,从多方面综合评估其临床效果,为抑郁症患者的治疗提供新思路.     

α-吡啶甲酸铜(II)配合物的室温固相合成

以α-吡啶甲酸和乙酸铜为原料,用室温固相反应合成了α-吡啶甲酸铜Cu(C5H4NCOO)2.2H2O,用元素分析、X射线粉末衍射、红外光谱和热分析等方法对产物进行表征。X射线粉末衍射数据指标化计算证实其晶体结构属于单斜晶系,晶胞参数为:a=1.382 1 nm,b=1.230 8 nm,c=0.727 2 nm,β=93.68°。表征结果表明,α-吡啶甲酸的羧基中的羟基氧原子和杂环氮原子及水分子中的氧原子参与配位,形成了配位数为6的配合物。     

Spectroscopic and conformational study of chitosan acid salts

The efficient procedure for preparation of chitosan acid salts in isopropyl alcohol under mild condition has been demonstrated. The salts were prepared by dissolving chitosan into ascorbic acid, p-amino benzoic acid and p-nitro benzoic acid, respectively, and then washed with an isopropyl/water mix-solvent. The prepared crystal salt and molecular conformation of modified chitosan derivatives are characterized by using ultraviolet, Fourier transform infrared (FTIR), ¹H nuclear magnetic resonance (NMR), X-ray diffraction and Circular dichroism (CD) techniques. The formation of salts was confirmed by FTIR (∼1,523–1,557 cm⁻¹) and NMR (∼7–8 ppm) with respect to the bonding between NH₂ group on chitosan and COOH group on acid. The CD spectra of chitosan salts showed negative at (253, 285 and 295 nm band) in chitosan ascorbic acid, p-amino benzoic acid and p-nitro benzoic acid salt respectively in DMSO, indicating that the polymer adopted a helical secondary structure. The polymers are highly soluble in a wide pH range, which opens new perspectives for the biomedical application of chitosan based-materials.     

Influence of ammonium salt formation on the activity and selectivity of the 12-molybdophosphate heteropolyacid catalyst prepared by solid–solid interaction in the ammoxidation of 2-methylpyrazine

The ammonium salt of 12-molybdophosphoric acid has been prepared by the solid-state interaction of the ammonium salts of molybdenum and phosphorus. The catalysts obtained by pretreatment of the precursor at various temperatures, have been characterized by nitrogen adsorption, X-ray diffraction (XRD), Fourier-transformed infrared (FTIR) spectroscopy and temperature-programmed decomposition (TPD) of the catalysts. Ammoxidation of 2-methylpyrazine has been carried out on these catalysts. The amount of ammonium salt present in the catalyst has been correlated with the activity and selectivity of the catalysts.     

氟硅酸钾在稀硫酸溶液中溶解度的测定与关联

湖北某化工公司将磷酸生产过程中的废水及磷石膏固结排出的渗水进行收集并循环利用,冬天废水中的无机盐类结晶堵塞泵体和输送管道,影响废水循环利用系统的正常运行。经分析结晶物主要成分是氟硅酸钾等难溶盐。采用平衡法测量了0~40 ℃内,氟硅酸钾在pH为1.5~3.5时稀硫酸溶液中的平衡溶解度,并采用Apelblat经验方程对氟硅酸钾平衡溶解度与温度做了关联,为废水中氟硅酸钾等难溶盐的结晶动力学研究提供了基础物性数据。研究结果表明：1）随着pH的降低或温度的升高,氟硅酸钾的溶解度增加;2）Apelblat经验溶解度方程能较好地关联氟硅酸钾平衡溶解度与温度。     

加料顺序对两种盐溶解性的影响

盐的溶解及盐效应的研究对化工技术开发具有重要意义。采用平衡法,常压下,测得了对苯二甲酸二钠在不同温度下于水中的溶解度。在常压和298.15 K下,考察了对苯二甲酸二钠等7种有机盐和无水硫酸钠等3种无机盐在水中的两两溶解过程,发现加料顺序会影响两种盐的溶解性。得到如下结果:先溶解难电离的盐再溶解易电离的盐,则后者的溶解速度变化不明显;而先溶解易电离的盐再溶解难电离的盐,则后者的溶解速度会显著降低且溶解度变小。将其中一种盐的量固定后,在一定时间内另一种盐所能溶解的量定义为准溶解度。测定了对苯二甲酸二钠在不同浓度的柠檬酸三钠水溶液中的准溶解度,为相关化工行业的产品分离纯化提供依据。     

Mixed salts—scaling limits and propensity

The main aim of desalination is removal of dissolved species from water either by thermal or membrane processes. In either process, the saline solution becomes concentrated, and once the concentration of salts exceeds its saturation limit, they form an unwanted deposit referred to as a fouled or scale layer. Even though precipitating salts coexist in industrial water systems, due to the complexity of the fouling process, research has primarily been concentrated on a single salt precipipation. The effect of other ionic species has been taken into account through the solution's ionic strength and use of the Debye Huckle Theory or a modified version of that. This paper critically assesses the current practices and consolidates the recent and ongoing work done by the author and her students [1-5] in thermodynamics and scaling limits in mixed salt solutions. The results indicate that the thermodynamics of single salt crystallization are not applicable to practical conditions of feed water when mixtures of salts are present. It is shown in various systems that the interactive effects of coexisting salts and the presence of a common ion cannot be ignored. Co-precipitation of salts with or without a common ion affects the solubility constants of the salts, and therefore application of the solubility data obtained under a single salt precipitation are questionable in mixed salt precipitation. Even the presence of minute amounts of another precipitating salt affects the thermodynamics and the scale structure and strength, which renders inapplicable the solubility data for the pure salts. The effect depended on both the dominance and type of salt. It should be emphasized that these results were obtained despite the fact that these assessments took into account the effect of solution ionic strength. Thus, considering the effect of ionic strength—though necessary—is not sufficient in mixed solutions. The presence of one salt does indeed affect the structure of the other salt. The effect of other salts on the scale morphology should not be ignored, and the author hypothesizes that to be the reason for inapplicability of the pure salt thermodynamics to that of mixed solutions. This paper establishes through thermodynamic relationships and through the Gibbs free energy of formation that the thermodynamic solubility constant of a salt in pure solution is different from that in a mixed solution if the morphology is affected by the presence of other salts.     

水飞蓟宾与水杨酸、丁香酸、水杨酰胺的共晶

水飞蓟宾在水和脂质介质中溶解性较差，生物利用度低，而药物共晶给药技术可在不改变药物药效的前提下提高药物溶解度、溶出速率、生物利用度和稳定性等理化性质。采用溶剂蒸发法在不同溶剂中成功制备出水飞蓟宾-水杨酸、水飞蓟宾-丁香酸、水飞蓟宾-水杨酰胺3种共晶。通过X-射线衍射、傅里叶变换红外光耦等表征手段确定了共晶的形成，且对3种共晶进行溶解度测定，结果表明3种共晶增加了水飞蓟宾在水中的溶解度。     

Agomelatine co-crystals with resorcinol and hydroquinone: Preparation and characterization

We prepared and characterized co-crystals of the antidepressant drug agomelatine with pharmaceutically acceptable coformers for enhanced solubility. A novel agomelatine-resorcinol (AGO-RES, 2 : 1) co-crystal was synthesized and its crystal structure was confirmed via single crystal X-ray diffraction. The AGO-RES co-crystal structure was created through the O-H???O and N-H???O hydrogen bonding between the phenolic OH of RES and the amide group of AGO. The chemical structure of two AGO co-crystals was characterized by FT-IR and Raman spectroscopies, whereas the solution behavior was determined by the intrinsic dissolution rate. When tested in water, both AGORES and AGO-HYQ form-I co-crystals showed higher apparent solubility than pure AGO. But the resulting AGO solution in a supersaturated state partially precipitated into specific crystal forms of AGO. As anticipated, the intrinsic dissolution rate of AGO was substantially enhanced by the co-crystal forms, which signifies that the bioavailability of AGO can be increased via co-crystal formulation approach.     

Synergistic effect of salt ions and water-soluble amphiphilic compounds of acidic crude oil on surface and interfacial tension

This study investigated the effect of solubility of amphiphilic compounds of acidic crude oil in water on the surface and interfacial tension (IFT) with NaCl, MgCl₂, CaCl₂, and Na₂SO₄ salts. Accordingly, distilled water, along with the salts mentioned in zero ionic strength up to 2 mol were put in contact with crude oil to become saturated with amphiphilic compounds. The effects of these compounds were investigated on the properties of contact water by pH, total organic carbon (TOC), FTIR (Fourier transform infrared spectroscopy), water-air surface tension (ST), and water-n-decane IFT tests. The results showed that some of the organic components of crude oil, especially acidic and basic compounds, are present or soluble in water, which have a significant effect on reducing the surface and IFT. The IFT reduction of water-n-decane was greater than the water-air ST system. Also, the observations showed that for both NaCl and Na₂SO₄ salt water, with increasing ionic strength of water, there was an optimum salinity within the range of 0.1-0.25 mol/L for both salts with the amount of surface and IFT minimized at this point. In the other two salts, this point was delayed upon elevation of ionic strength and was observed at high salinity. In this case, divalent cations reduce tension rate compared to monovalent cations. Due to solubility of acidic and basic groups in water, pH of salt water illustrates an acidic trend. Results of the FTIR test confirmed solubility of these compounds as well.     

羟基乙烷磺酸钙的合成及表征

以β-巯基乙醇和H2O2溶液为原料合成了羟基乙烷磺酸（ITA）,用ITA和CaCO3为原料合成了目标产物羟基乙烷磺酸钙[Ca（HOCH2CH2SO3）2.2H2O],其结构经TGA,FT-IR1,H NMR和元素分析表征。利用热重分析研究了羟基乙烷磺酸钙的热分解过程,在动态空气气氛下,其热分解过程分为两个阶段。第一阶段（30~300℃）失重率为11.06%,失重主要由所含结晶水引起,结晶水的个数为2。第二阶段（300~650℃）失重率为46.16%,这一阶段是其主要分解过程。通过红外光谱确定了羟基乙烷磺酸钙的热分解产物为CaSO4。25℃羟基乙烷磺酸钙在水中的溶解度为120g.100g-1。     

Low-temperature fabrication of porous ZrC/C composite material from molten salts

In this work, biological ceramic-wood porous ZrC/C materials were prepared in a KCl-KF molten salt reaction medium, using Zr as a metal source and a C template as C source. The effects of reaction temperature and salts/Zr mole ratio on the formation of porous biomorphic ZrC/C ceramics were investigated. The phase compositions and morphological structures of the C templates and porous ZrC/C ceramics were characterized by X-ray diffraction, Raman spectroscopy, scanning electron microscopy, transmission electron microscopy, thermogravimetric analysis, and pore size analysis. The results showed that the ZrC grains were equiaxed and enhanced the oxidation resistance of the material. Furthermore, a possible reaction mechanism for the formation of porous biomorphic ZrC/C ceramics in molten salt is proposed.